超高效液相色谱-串联质谱法同步测定贝类水产品中4种脂溶性藻毒素

Simultaneous determination of 4 types of lipophilic algae toxins in shellfish products using ultra performance liquid chromatography tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  贝类产品  脂溶性藻毒素  电喷雾电离  正负离子模式  同时监测

英文关键词:ultra performance liquid chromatography tandem mass spectrometry  shellfish products  lipophilic algae toxins  electrospray ionization  positive and negative ion mode  simultaneous determination

中文摘要:

      目的 建立一种超高效液相色谱-串联质谱法同时测定贝类产品中4种脂溶性藻毒的方法。方法 样品采用甲醇均质提取, 用HLB小柱净化, 在乙腈-5 mmol/L醋酸铵水溶液体系中, 经Kinetex C18柱(150 mm×3 mm, 2.6 μm)梯度洗脱, 实现了4种藻毒素的良好分离。采用了电喷雾正负离子同时监测模式对4种脂溶性藻毒素进行外标法定量测定。结果 目标化合物的检出限为2.3～20.7 pg/g, 在3.8～1378.0 pg/g浓度范围内线性良好, 相关系数r2在0.99407~0.99923之间, 同时以贝类产品为基底的4种化合物在高、中、低3个加标水平浓度下的回收率为70%~95%, 相对标准偏差(relative standard deviation, RSD)为2.3%~7.7%。结论 该方法灵敏、准确、高效, 适合用于贝类水产品食用安全的日常风险监测项目中。

英文摘要:

      Objective To establish a method for simultaneous determination of 4 kinds of lipophilic algae toxins in shellfish products using ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Methods Samples were first extracted by methanol, followed by a purification using an Oasis HLB SPE column. Further separation of the 4 targets compound was achieved on a Kinetex C18 column (150 mm×3 mm, 2.6 μm) via UPLC by gradient elution with acetonitrile and 5 mmol/L ammonium acetate aqueous solutionas mobile phase. Quantification of the 4 targets was performed on a mass spectrometry, which simultaneously carried out by means of electrospray ionization in positive (ESI＋) and negative ion mode (ESI-) mode with an external standard. Results The method showed a good linearity in the concentration range of 3.81378.0 pg/g, with the detection limits of 2.320.7 pg/g. The correlation coefficients (r2) were between 0.994070.99923 for 4 toxins. The average recoveries for the high, medium and low concentrations of external standard were between 70%95% with the relative standard deviations(RSD) 2.3%7.7%. Conclusion The method is sensitive, accurate, with high efficiency and is suitable for the daily risk monitoring project of shellfish food safety.